CN1277570A - Method of manufacturing metal powder - Google Patents

Method of manufacturing metal powder Download PDF

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Publication number
CN1277570A
CN1277570A CN99801403A CN99801403A CN1277570A CN 1277570 A CN1277570 A CN 1277570A CN 99801403 A CN99801403 A CN 99801403A CN 99801403 A CN99801403 A CN 99801403A CN 1277570 A CN1277570 A CN 1277570A
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CN
China
Prior art keywords
comb
metal dust
cooling liquid
nozzle ring
liquid
Prior art date
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Granted
Application number
CN99801403A
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Chinese (zh)
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CN100364700C (en
Inventor
菊川真利
松永繁昌
稻叶恒太
岩津修
武田彻
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Fukuda Metal Foil and Powder Co Ltd
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Fukuda Metal Foil and Powder Co Ltd
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Priority claimed from PCT/JP1998/005867 external-priority patent/WO1999033598A1/en
Application filed by Fukuda Metal Foil and Powder Co Ltd filed Critical Fukuda Metal Foil and Powder Co Ltd
Publication of CN1277570A publication Critical patent/CN1277570A/en
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Publication of CN100364700C publication Critical patent/CN100364700C/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086Cooling after atomisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/088Fluid nozzles, e.g. angle, distance
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0884Spiral fluid

Abstract

The present invention relates to a method for preparing metal powder by means of blowing a cooling liquid toward a flowing down melt metal flow characterized that the cooling liquid is successively discharged downwardly from an annular nozzle toward the melt metal flow for surrounding it in the form of a hyperboloid of one sheet, wherein the annular nozzle is provided with a hole through which the melt metal flow may pass, and that the hyperboloid of one sheet has a pressure reduced by 50 to 750 mmHg at the neighborhood of the constricted part inside the hyperboloid of one sheet. According to the present invention, there may be prepared fine and sherical metal powder which has a narrow range of a particle size distribution.

Description

The method for preparing metal dust
The present invention relates to a kind of method for preparing metal dust, relate to a kind of trickle and spherical metal dust of prepared sizes narrowly distributing particularly.
The preparation metal dust has several methods, and one of them is known atomization method, and it is that a kind of cooling medium (or atomizing medium) is blowed to motlten metal flowed with effective method for preparing metal dust.Atomization method is classified as the gas atomization method of using gases cooling medium usually and uses the atomization of liquid method of liquid cooling medium.
The for example known utilization of gas atomization method is at United States Patent (USP) 1,659,291 and United States Patent (USP) 3,235,783 in the method that atomizes of disclosed nozzle.But can not observe the gas jet of discharging according to this gas atomization method, utilize the Schlieren photography to observe mobile dull expansion of proof gas jet from nozzle.It is believed that gas jet is a compressible fluid, in adiabatic expansion after the nozzle ejection.Because adiabatic expansion makes the energy density of gas jet sharply reduce, be difficult to effectively obtain trickle metal dust by the gas atomization method.Zhi Bei metal dust has wide size distribution like this.In addition, also there is another problem in the gas injection method, and air may be involved in the gas jet that will blow motlten metal.
Yet, having low relatively cooling capacity as the gas of cooling medium, the motlten metal that is disperseed by gas jet drips and can self become the curing of spherical back like this.Therefore, normally spherical according to the metal dust of this gas atomization method preparation.
Disclosed nozzle has one at the gas access of nozzle tangential direction and the blade in nozzle in above-mentioned United States Patent (USP) 1,659,291 and United States Patent (USP) 3,235,783, so that the gas jet of discharging is directed into the direction close with the tendency of nozzle central authorities.It is believed that this tendency can avoid gas to be involved in the gas jet, motlten metal just can not upwards be blowed like this.
On the other hand, the V-jet type atomization of liquid method (as Figure 11 (a) or Figure 11 (b) shown in) of known atomization of liquid method as it is characterized in that liquid jet is being assembled in the line, it is characterized in that circular cone-jet type atomization of liquid method (shown in Figure 11 (c)) that liquid jet is assembled at a point, it is characterized in that pencil-jet type atomization of liquid method (shown in Figure 11 (d)) of assembling on one point from the liquid jet that pencil jet type nozzle segment 14 is discharged.
Because the cooling medium that in atomization of liquid method, uses be a kind of can not compressed fluid, be used for disperseing the energy density of liquid jet of motlten metal stream 6 more much bigger than the gas jet.Therefore, atomization of liquid metal dust is much trickleer than the gas atomization metal dust.
Yet there is a problem in the atomization of liquid method of prior art, and liquid jet is assembled or collision at a line or a point.Therefore, the motlten metal that disperseed before solidifying just drips and must concentrate near focus, and acutely passes liquid jet, thereby is cooled off suddenly.Therefore the motlten metal that disperses drip with bunch form contact with each other and adhere to together, the metal dust of Huo Deing just has irregular shape and comprises the wide size distribution of crude metal powder like this.
Therefore, if required metal dust has spherical shapes and narrow size distribution, must be in addition with other separation or mechanical treatment, thereby improved manufacturing cost.
Several improving one's methods of addressing the above problem are arranged in atomization of liquid method.
A kind of improving one's methods is that less V-jet in the elevation angle or circular cone jet are assembled, thereby reduces the collision energy of liquid jet, thus the distortion that the metal that reduction disperses drips.Yet in fact the metal dust of Huo Deing does not have spherical shapes.And, because improving one's methods, this make the distance between nozzle and the focus strengthen, will lose lot of energy, and such coarse grain metal dust that obtains just has the size distribution of broad.
At Japan Patent No.552,253 (Japanese patent application publication No. No.43-6,389), Japanese patent application publication No. 3-55 discloses improving one's methods of several circular cone jet type atomizations of liquid in 522 and Japanese patent application publication No. 2-56,403.According to being disclosed in Japanese Patent No. 2-56,403 invention imports cooling medium and to discharge liquid jet with the tangent line of nozzle or normal direction.If there is the situation of pore-forming in the liquid of discharging, can only prepare the metal dust of coarse grain.
At Japanese patent application publication No. No.53-16,390 disclose another kind improves one's methods, and provides one to be used for making the comb of liquid jet turbulent flow to improve the efficient of disperseing motlten metal stream in the bottom surface.According to originally improving one's methods, motlten metal stream and turbulent flow jet acutely contact preparing trickle metal dust, but metal dust is not spherical.
At Japanese publication publication number No.1-123,012 discloses a kind of nozzle ring of Scrawl, with the form discharge ring of the hyperbolic surface layer cooling medium around motlten metal stream.Discharge the periphery of liquid jet from the nozzle ring that is used for disperseing with the motlten metal stream of the process hyperbolic surface layer constriction of pruning continuously.Therefore, it is adhering to each other that this nozzle can prevent that the motlten metal that disperses from dripping, thereby prepare trickle spherical metal dust.Yet, because disperse the efficient of motlten metal stream very low, to such an extent as to a part of motlten metal stream is not just disperseed to produce through the constriction of hyperbolic surface layer the metal dust of coarse grain.Therefore, just the metal dust of 012 disclosed round nozzle prepared sizes narrowly distributing can not be passed through veritably at the unexposed patent publication No. No.1-123 of Japan.
It is trickleer and have more the metal dust of spherical form to the purpose of this invention is to provide a kind of effective preparation, and its particle diameter metal dust for preparing than the atomization of liquid method in the existing metal that distributes is narrow.
In order to overcome the problems referred to above, the inventor studies and has finished the present invention.Provide a kind of by cold liquid being blown into the method for preparing metal dust in the motlten metal stream that flows downward, it is characterized in that cooling liquid flows to motlten metal stream downwards continuously from nozzle ring, flow around motlten metal with the bi-curved formal ring of one deck, wherein nozzle ring has the hole that a motlten metal stream can pass through, and near the constriction of this layer hyperboloid the inside, bi-curved pressure reduces by 50~750mmHg.
Therefore, flow by liquid jet is sprayed to the motlten metal that flows downward with the bi-curved form of one deck, and solve the above problems in the very big pressure differential of the inside of hyperbolic surface layer generation.The pressure that reduces in the hyperbolic surface layer has several method.For example, can be placed in comb the lower position of nozzle ring hereinafter described, use the chamber that less inner volume is arranged, or a preferred pumping equipment is installed in the chamber.
Be detailed description of the present invention below.
The accompanying drawing summary
Fig. 1 is cross-sectional view (a) and the longitudinal sectional view (b) that is placed in the nozzle ring that is moving on the device of the present invention that is used for preparing metal dust.
Fig. 2 is the perspective view of the liquid jet of discharging from nozzle ring with bi-curved form in Fig. 1.
Fig. 3 is the figure of another embodiment of nozzle ring of the present invention.
Fig. 4 is the figure of another embodiment of nozzle ring of the present invention.
Fig. 5 to 7 is comparisons that the pressure that produces in the hyperbolic surface layer of discharging from various nozzles or the circular cone changes.
Fig. 8 represents is relation between the metal dust intermediate value of the vortex angle of liquid jet and acquisition.
Figure 10 with Electronic Speculum amplify according to the present invention and the metal dust of prior art.
Figure 11 represents is various atomization of liquid method figure according to prior art.
That Figure 12 represents is the figure of another embodiment of nozzle ring of the present invention.
Fig. 1 uses the present invention to prepare the embodiment of nozzle ring of the method for metal dust, and specifically, (a) expression is a cross-sectional view, and (b) expression is longitudinal sectional drawing at the y of (a) axle. The nozzle 1 that represents in Fig. 1 is positioned in one and is used for preparing on the device of metal, and the metal flow 6 that flows down like this can be by the hole 2 that forms in nozzle ring.
Nozzle ring has entrance 3, vortex chamber 4, narrow annular channel 5 and comb 21. Cooling liquid is introduced from entrance 3, in vortex chamber, formed eddy current, from narrow annular channel 5, discharge, the flow through flow of molten metal in hole 2 of directive. Describing in further detail about this nozzle ring 1 below.
Entrance 3 is positioned in the tangential direction of the vortex chamber 4 in the nozzle ring, can import cooling liquid in the vortex chamber 4 like this. Although it is enough that an entrance is provided in nozzle ring of the present invention at least, provide in this embodiment two entrances under higher pressure, to guide cooling liquid. Entrance also needn't be placed in the tangential direction of vortex chamber, and can be formed at the normal direction of vortex chamber.
Vortex chamber 4 is the peripheries that form to come around the hole 2 of nozzle ring 1. Therefore, before cooling liquid is released, cooling liquid is imported in the minor air cell 4, form eddy current, around the flow of molten metal that flows out by hole 2. Vortex chamber 4 has a cavity space 7, and 4 peripheries do not have obstacle in the chamber, and the cooling liquid that imports from entrance so generally can be dispersed in the vortex chamber. Therefore cooling liquid just can under high pressure import in the nozzle ring. If at tangential method two or more entrances 3 are arranged at nozzle, just can omit chamber 7.
In the chamber 7 of vortex chamber 4, provide several blades 8.Blade 8 is used for stablizing cooled liquid stream, can make cooling liquid more near the vortex the inside like this.Any point of the narrow annular channel 5 (diameter 20mm) that cooling liquid is formed from 2 the inner surface along the hole under constant compression force normally discharges then.The angle that forms between the tangential direction of spout radius direction and blade upper outside is 3 °≤ω 0≤ 90 °, 5 °≤ω preferably 0≤ 90 °, be more preferably 7 °≤ω 0≤ 90 °, liquid jet can discharge with the preferable range of described vortex angle ω hereinafter like this.
In addition, also can provide another kind be can be used to make cooling liquid form eddy current and described blade at vortex chamber by the approach of rotations such as rotary press or passage uses together or replaces blade.
Cooling liquid obtains to be directed into narrow annular channel 5, further the cavity space 7 ' mesoscale eddies that is being positioned at blade in vortex chamber 4 mesoscale eddies power.Cavity space 7 ' in vortex chamber 4 becomes more and more narrow towards narrow annular channel 5.Thereby cooling liquid is with 100 meter per seconds or bigger, preferably 130 meter per seconds or bigger flow velocity, be more preferably 200 meter per seconds or bigger flow velocity is emitted from narrow annular channel 5, the speed of liquid jet can be used in the cooling fluid calculation of pressure of the importings that inlet 3 measures by the BernoulliShi theorem.
Must spray to motlten metal stream to liquid jet after by hole 2, narrow annular channel does not limit to the inner surface that is positioned at the hole, but can be positioned at the lower surface of nozzle ring.According to the present invention, the form of narrow annular channel is not limited to circle shown in the drawings, and can be oval, rectangle etc.
Can take the bi-curved form of one deck shown in Figure 2 from the liquid jet 13 that nozzle ring 1 is discharged.There are several streamlines 10 to show at individual layer hyperboloid illustrated in figures 1 and 2 from the direction of the liquid jet of any point of narrow annular channel 5 ejection.According to the present invention, can flow from the liquid jet 13 (or every streamline 10) of narrow annular channel 5 any points ejections forms constriction 11, and it is at first assembled without collision like this, disperses then.Individual layer hyperboloid constriction can not be observed sometimes, especially works as liquid jet and flows with turbulent flow or with following less vortex angle ω.When the vortex angle of the streamline of reading from liquid jet is 1 ° or when bigger, it seems to obtain preferred effect according to the present invention.
Liquid jet preferably sprays with following vortex angle ω and angle of depression θ from nozzle ring of the present invention.
The speed V of liquid jet can be divided into along the velocity component V of narrow annular channel tangential direction (as the x direction of principal axis among Fig. 4) x, at the velocity component V of narrow annular channel normal direction (as the y direction of principal axis among Fig. 4) y, and the velocity component V of vertical direction z(as the z direction of principal axis among Fig. 3).Then the vortex angle is defined as y axle and V xAnd V yAngle between the direction of the power that produces.Angle of depression θ is defined as z axle and V yAnd V zAngle between the direction of the power that produces.
The vortex angle of preferred liquid jet is 1 °≤ω≤20 °, is more preferably 2 °≤ω≤15 °, most preferably is 3 °≤ω≤10 °, and preferred angle of depression θ is 5 °≤θ≤60 °, is more preferably 7 °≤θ≤55 °, most preferably is 8 °≤θ≤40 °.Liquid jet in above-mentioned vortex angle ω and the ejection of angle of depression θ scope can produce good especially metal dust.
This nozzle is provided with a comb 21, and the internal diameter of comb 21 is generally close with the internal diameter of the arbitrfary point of nozzle ring, and stretches out downwards from the lower surface of the nozzle ring shown in Fig. 1 (b).For example the metal or the porcelain of maximum hardness are worn to prevent it preferably to provide one deck coating at the inwall of comb.Comb 21 is positioned on the nozzle ring, and the axis of nozzle ring can be consistent with the axis of comb like this, makes liquid discharge the hyperbolic surface layer that is formed on the comb 21 from nozzle slot 5.Thereby can produce significant big pressure differential in the inside of hyperbolic surface layer.
According to the present invention, length from the hyperboloid top edge to constriction is defined as " l ", the 0.5l scope is called as " close region of hyperbolic surface layer constriction " about the constriction central authorities in the hyperbolic surface layer, and near the pressure the inlet in nozzle ring hole is called as " pressure of atomization of liquid environment " (with reference to Fig. 5).The close region of the constriction of hyperbolic surface layer is than the little 50-750mmHg of pressure in atomization of liquid zone, and preferably 100-750mmHg is more preferably 150-700mmHg, most preferably is 200-700mmHg.And then the close region on hyperboloid top is by the strict hyperbolic surface layer top edge scope of 0.5l up and down that is limited in, preferably than the little 10-100mmHg of pressure of atomization of liquid environment.In addition, constriction than lower part, be limited in " close region of hyperbolic surface layer constriction " by strictness, preferably than the low 50-700mmHg of the pressure of atomization of liquid environment.So big pressure differential in the hyperbolic surface layer can strengthen the efficient of disperseing motlten metal stream, so just prevents that it from not disperseed just to pass through constriction.
Be placed in nozzle ring of the present invention comb the size and unrestricted.Yet when the length of comb is defined as " L ", the internal diameter of comb is defined as " R ", and the diameter of narrow annular channel 5 is for being defined as " r ", and the length L of comb is preferably 3-100r, 5-50r more preferably, and internal diameter R is preferably 1.5-5r, more preferably 2-4r.
As shown in Figure 3, comb is mounted the dry tube diameter rectification body 22 bigger than the diameter of constriction 11, and the top 26 of main is just along the positioned internal of hyperbolic surface layer than lower part like this.Rectification body 22 prevents liquid jet and the collision of comb internal diameter, and liquid stream just can not become the upper reaches from turbulent flow like this.Rectification body 22 plays the effect of the sectional area that is reduced in the comb lower part, and then is reduced in the pressure of hyperboloid constriction 11 or lower 32.Rectification body can have for example column type of different shape, column type, and tapered or truncated cone type is installed in the comb by a fixator 28, and fixator 28 puts in the radial direction of comb from inwall.In addition, can be fixing with the fixator 28 ' that goes out deeply from the comb outside.
There is the comb of above-mentioned rectification body that the length identical with the comb that does not have rectification body can be arranged, although can long 3-30r, preferably 5-20r.
Shown in the dotted line of Fig. 3, can further provide a gas inlet pipe 24 to comb, this pipe 24 has a valve 29, is used for being adjusted at the pressure in the comb.Gas inlet pipe 24 can make gas (or atmosphere) be imported into simultaneously in the comb when liquid jet, is controlled at pressure or liquid jet flow condition in the comb like this, thereby preventing that offgas duct is worn or adheres to motlten metal drips.Can unlatching or the size of valve-off and adjustment gas inlet pipe, configuration direction and allocation position are controlled the importing of gas to comb.Also can provide hair-dryer to force air is injected in the comb, so further be reduced in the pressure in the comb in gas inlet pipe.
The internal diameter of comb 21 is not limited at the diameter of its any point similar.As shown in Figure 4, comb can have the parts part 36 of inclination, and the longitudinal section of tilt component part is extended downwards and separated with axis by the axis of comb.Tilt component partly relaxes or prevents the collision of liquid jet and comb inwall, and the metal dust of Huo Deing has less distortion like this, and the destruction of year old comb inwall has also been slowed down.
As shown in Figure 4, the angle φ that preferred angled loses part 36 is to 5 °≤φ of vertical direction≤60 °, and this angle φ preferably is set than little 5-20 ° of above-mentioned angle of depression θ.
In addition, use the comb that the tilt component part is arranged preferably to follow with described rectification body 22 configurations.This have the comb of rectification body that the length identical with there not being the rectification body comb can be arranged, although preferably include long 3-30r, more preferably 5-20r.
Except described tilt component part 36 is provided to comb, can use the comb of the tilt component of the axis of several longitudinal sections by comb as shown in figure 12, comprise first tilt component part 36 of stretching out downwards away from axis, first vertical member part 37 that lower part from the first tilt component part 36 stretches vertically downward, one is stretched the second tilt component part 36 ' near axis and second a vertical member part 37 ' of extending vertically downward from the second tilt component part, 36 ' lower end from first vertical member part 37 lower ends downward.Therefore the comb that has the tilt component part of described downward extension has a plurality of internal diameters, and at first expansion reduces then gradually.There is the comb of several tilt component parts can not provide rectification body.The angle φ ' that forms between tilt component part 36 ' and vertical direction can be different with above-mentioned angle φ, although preferred close with it.
Although water can be discharged from nozzle with various volumes, preferred " at the motlten metal stream of unit interval " volume is 1 with the ratio of " the cooling fluid volume of the discharge of unit interval ": 2-100, more preferably 1: 3-50, most preferably 1: 5-30.Therefore, can be effectively and prepare the good metal powder economically.
The present invention is not limited to the nozzle ring that narrow annular channel 5 is arranged as shown in Figure 1.For example, jet element 14 (Fig. 7 (d)) that can the several pencil jet types of annual configuration, its outlet be along narrow annular channel shown in Figure 15 orientations, and the jet element of each pencil jet type can be discharged with the form of the hyperbolic surface layer consistent with streamline 10 like this.In this case, the pencil jet type jet element of annual configuration comprises according to nozzle ring of the present invention.
The device that is used for preparing metal dust with nozzle ring 1 can effectively produce trickleer and spherical metal dust, and the particle diameter of this metal dust distributes narrower than the prior art.But the present invention is not limited to a concrete aspect, the mark of motlten metal stream is not only and is resembled prior art and collide with liquid jet, and follows following mechanism and make trickle metal dust.
According to the present invention, can not have high energy density by compressed liquid jet, to discharge liquid jet with the form of hyperbolic surface layer and do not assemble with steady flow, the hyperbolic surface layer that forms in comb is in constriction 11 or the pressure of unexpected reduction is arranged than lower part 32.Therefore, when motlten metal stream 6 flows to constriction 11, thereby its is attracted flow rule ground and dispersion continuously by general constant energy before dripping produce trickle motlten metal by constriction.
The motlten metal of the dispersion of gained drips and to shift to than lower part 32 by constriction 11 and is solidified into metal dust.According to the present invention, motlten metal drips relatively placidity ground cooling before curing, subsequently without the front of hyperbolic surface layer with by the surface tension balling-up.On the contrary, the focus that the motlten metal that disperses according to the atomization of liquid method of prior art drops in liquid jet contacts with each other, and and acutely contact and is passed through liquid jet by cooling rapidly, and this is and the remarkable different improved place of the present invention.
The metal that the present invention can be applied to any kind of is metallic element, metallic compound, metal alloy and intermetallic compound for example.According to the present invention, prepare the metal dust that described characteristic is arranged by regulating the atomization condition that is fit to metallic character.
Metal dust preferred characteristics by the present invention's preparation is as described below.Except special interest, the particle diameter that the atomizing according to the present invention is described below is 1mm and with JISZ-8801 can less separating metal powder.
1. the metal dust with the present invention preparation preferably has superficial density than being 28% or more, and especially 30% or more, be more preferably 32%.
2. the metal dust with the present invention preparation preferably has bulk density than being 45% or more, and especially 50% or more, be more preferably 50% or more.
3. preferably to have median diameter be 50 μ m or littler to metal dust, and especially 35 μ m or littler are more preferably 25 μ m or littler, most preferably are 15 μ m or littler.
4. median diameter is the fine-powder that 25 μ m or littler metal dust preferably can include following particle diameter and following concentration.
1) preferably exist particle diameter be 10 μ m or more small concentration be at least 20 weight % or more, especially 40 weight % or more 45 weight % more preferably or more fine-powder.
2) preferably exist particle diameter be 5 μ m or more small concentration be at least 3 weight %, 10 weight % or especially are more preferably 18% weight or more fine-powder more.
5. median diameter is the fine-powder that 15 μ m or littler metal dust preferably can include following particle diameter and following concentration.
1) preferably exist particle diameter be 10 μ m or more small concentration be at least 35 weight % or more, especially 45 weight % or more 50 weight % more preferably or more fine-powder.
2) preferably exist particle diameter be 5 μ m or more small concentration be at least 10 weight %, 15 weight % or especially are more preferably 20 weight or more fine-powder more.
3) preferably exist particle diameter be 1 μ m or more small concentration be at least 0.01 weight %, 0.05 weight % or especially is more preferably 0.1 weight % or more fine-powder more.
6. the metal dust by the present invention preparation can have geometric standard deviation 2.5 or littler, and particularly 2.3 or littler, be more preferably 2.2 or littler, geometric standard deviation can be estimated the width that particle diameter distributes.
7. the metal dust of the present invention's preparation preferably has specific area 4000cm 2/ g or littler, particularly 3000cm 2/ g or littler is more preferably 2500cm 2/ g or littler.
Embodiment
Further describe the present invention in conjunction with the embodiments.The following examples are best way that the inventor carries out during using, but the present invention is not limited thereto.
Measured from the pressure variation of the liquid of each nozzle ring discharge.Pore with a sectional area ratio constriction little 20% of inserting along axis from hyperbolic surface layer top is measured pressure, and another pore of measuring the pipe of pressure like this links to each other with pressure gauge.
That Fig. 5 represents is the Scrawl nozzle ring A that comb is arranged according to of the present invention 1With the capable nozzle B of the vortex that does not have comb according to prior art 1, and the curve that changes according to the pressure in the hyperboloid of the tapered jet type nozzle ring C of prior art.
This figure shows nozzle ring A of the present invention 1Producing significant pressure in constriction falls.
That Fig. 6 represents is the Scrawl nozzle ring A that all lengths comb is arranged according to of the present invention 2And A 3With the capable nozzle B of the vortex that does not have comb according to prior art 1Hyperboloid in the curve that changes of pressure.
This figure shows the nozzle ring of comb A 2And A 3In constriction than the nozzle ring B that does not have comb 1Producing significant pressure falls.The A3 of nozzle ring is than nozzle ring A 2Longer comb is arranged, also have bigger pressure to fall.
What Fig. 7 represented is according to nozzle ring A of the present invention 4With the Scrawl nozzle ring B that does not have comb according to prior art 2Or B 3The pressure history that in the hyperbolic surface layer, produces of liquid jet.
This figure shows that comb can make the pressure in hyperboloid reduce.
Use nozzle ring of the present invention to make various Cu, Cu-10%Sn alloy, the metal dust of Cr-Ni-Mo alloy and Fe-Si-Co alloy.
The analysis item of describing in table 1 is that the particle diameter of selecting with JISZ8801 is carried out less than 1mm or littler metal dust.Table 1 also shows the result.The concrete grammar of these analyses is as follows.
Apparent density is measured with ISO-3923.
Bulk density is measured with ISO-3953.
The apparent density ratio calculates according to " apparent density "/density of solid * 100.
The bulk density ratio calculates according to " bulk density "/density of solid * 100.
The intermediate value of diameter of particle is to use MICRO TRAC to measure with laser diffraction method (volume %).If comprising particle diameter is that 250 μ m or more metal dust are measured with sieve the particle diameter of metal dust.
Measuring particle diameter with laser diffraction and scattering method (volume %) is 10 μ m or littler, 5 μ m or littler, 1 μ m or littler in whole metal dust the content of shared fine-powder.
Geometric standard deviation is to be used in the median particle size of acquisition " accumulative total of the metal of 50% diameter "/" accumulative total of 15.87% metal dust " to calculate.
Specific area is measured with the BET method according to the gas phase absorption process.
Oxygen content is measured with non--disperse INFRARED ABSORPTION detector.
Productive rate is the percentage by weight that the particle diameter 45 μ m that select with JISZ8801 or littler metal dust account for particle diameter 1mm or littler metal dust.
Take the Electronic Speculum micrograph with the ESEM that Hitachi Seisakusyo Co.Ltd. makes.
Result in table 2 confirms when influencing following characteristic with metal dust comparison the present invention of the same race.
According to the apparent density of embodiment of the present invention and bulk density height than the metal dust of prior art.And according to the relative apparent density and the height of relative bulk density of embodiment of the present invention than the metal dust of prior art.These results show that metal dust according to the present invention has more spherical form than the metal dust of prior art.
Median particle size according to metal dust of the present invention is littler than the median particle size of the metal dust of prior art.This result shows that metal dust according to the present invention is trickleer than the metal dust of prior art.
Metal dust according to the present invention comprises than the metal dust of prior art and more muchs trickleer powder.Especially, significantly different with prior art is, metal dust of the present invention comprises particle diameter 1 μ m and littler particle diameter, and this is clearly perception in the laser diffraction method.
Metal dust according to the present invention is by the metal dust that the nozzle ring that does not have comb prepares littler geometric standard deviation to be arranged at metal dust especially than prior art.This result shows that metal dust according to the present invention has narrower particle diameter than prior art and distributes.
Oxygen content according to metal dust of the present invention is lower than the prior art.This is considered to because globular metallic powder of the present invention has less surface area to have due to the reason of anti-oxidation.
Wanting of productivity ratio prior art of the present invention is high.This is considered to according to motlten metal stream liquid-jet rule of the present invention and disperses continuously, and the motlten metal of dispersion is not easy to contact with each other before dropping in steady cooling.
Watch metal dust of the present invention to have more sphere with the chart that Electronic Speculum is taken, do not have the corner.
In addition, can be with various vortexs angle is arranged, the liquid jet of discharging from nozzle ring of the present invention with 850Kgf/cm2 and 135l/min pressure prepares various Cu-10%Sn metal alloy powders, with the vortex angle of investigation liquid jet and the relation between the median particle size, the relation between vortex angle and apparent or the bulk density.These results are shown in Fig. 8 and 9.
These results show that the vortex angle is big more, and metal dust is just trickle more and have a sphere.
Table 1
Metal dust ???????????????????????Cu The Cu-10%Sn alloy
Embodiment number or to colon Implement 1 Implement 2 Contrast 1 Contrast 2 Contrast 3 Implement 3 Implement 4 Contrast 4 Contrast 5 Contrast 6
Atomization condition Inject cooling liquid pressure (Kgf/cm 2) ????80 ???400 ???85 ???375 ???80 ??205 ??830 ??100 ??935 ??150
Liquid jet speed (meter per second) ???125 ???280 ???129 ???271 ???125 ??200 ??403 ??140 ??428 ??300
The pressure of constriction (mHg) ??-320 ??-585 ???- ???- ???-50 ??-212 ??-670 ???- ???- ??-60
Vortex angle ω (°) ???14.1 ???5.44 ???0 ???0 ???9.8 ??4.1 ??5.4 ???0 ??0 ??14.7
Angle of depression θ (°) ???35 ???25 ???33 ???25 ???17 ??38.5 ??22 ??15.4 ??25 ??17
The volume of cooling liquid volume/motlten metal ???10 ???10 ???10 ???10 ???10 ??20 ??20 ??20 ??20 ??20
Be with or without comb Have Have Have Have No Have Have No Have No
The analysis result of the metal dust that obtains Apparent density (g/cm 3) ???4.5 ???3.5 ???3.4 ???2.8 ????4.2 ??3.66 ??2.91 ??3.30 ??2.49 ??3.6
Bulk density (g/cm 3) ???5.8 ???5.3 ???4.9 ???4.5 ????5.5 ??4.98 ??4.72 ??4.21 ??3.62 ??5.1
Apparent density is than (%) ???50.6 ???39.0 ???38.2 ???31.5 ????47.2 ??41.1 ??32.7 ??37.1 ??28.0 ??40.0
Bulk density is than (%) ???65.0 ???59.6 ???55.1 ???50.6 ????61.5 ??46.1 ??53.1 ??47.3 ??40.7 ??57.3
Median diameter (μ m) ???36.4 ???15.2 ???80.5 ???25.4 ????130 ??20.4 ??8.86 ??73.5 ??10.4 ??75.4
The ratio of the refining metallic powder in metal dust (%) 10 μ m or littler ????- ???46 ????- ???18 ?????- ???- ??57 ???- ??45 ???-
5 μ m or littler ????- ???19 ????- ???5 ?????- ???- ??26 ???- ??17 ???-
1 μ m or littler ????- ???0.11 ????- ???0 ?????- ???- ??0.39 ???- ??0 ???-
Geometric standard deviation ???1.99 ???2.11 ???2.65 ???2.79 ????3.21 ??2.00 ??2.15 ??2.97 ??2.24 ??3.1
Specific area (cm 2/g) ???370 ???1600 ???670 ???2200 ????420 ??1120 ??1900 ??560 ??2600 ??520
Oxygen content (%) ???0.15 ???0.11 ???0.12 ???0.25 ????0.32 ??0.07 ??0.09 ??0.09 ??0.16 ??0.27
Productive rate (%) ???58.6 ???95.6 ???37.3 ???78.2 ????30.1 ??69.8 ??98.3 ??42.1 ??87.9 ??20.5
The figure number of the powder that amplifies with Electronic Speculum ????- ????(a) ????- ????(b) ??????- ???- ????(c) ???- ???(d) ???-
Table 2
Metal dust The Cr-Ni-Mo alloy The Fe-Si-Co alloy
Embodiment number or to colon Implement 5 Implement 6 Contrast 7 Contrast 8 Contrast 9 Implement 7 Implement 8 Contrast 10 Contrast 11 Contrast 12
Atomization condition Inject cooling liquid pressure (Kgf/cm 2) ??500 ??720 ??255 ??720 ??200 ??855 ????720 ???800 ??200 ??200
Liquid jet speed (meter per second) ??313 ??376 ??224 ??376 ??198 ??409 ????376 ???396 ??198 ??198
The pressure of constriction (mHg) ??-610 ?-620 ???- ???- ??-70 ??-594 ????-580 ????- ???- ??-70
Vortex angle ω (°) ??10.2 ??3.7 ???0 ???0 ??9.0 ??8.13 ????7.5 ????0 ???0 ???7.7
Angle of depression θ (°) ???25 ??15 ???25 ???9 ??15 ??35 ????20 ????25 ???18 ???16
The volume of cooling liquid volume/motlten metal ???40 ??40 ???40 ???40 ??40 ??30 ????30 ????30 ???30 ???30
Be with or without comb Have Have Have No No Have Have Have No No
The analysis result of the metal dust that obtains Apparent density (g/cm 3) ??2.79 ??2.53 ??2.34 ??1.77 ??2.5 ??1.69 ????1.82 ???1.19 ??1.50 ???1.8
Bulk density (g/cm 3) ??4.88 ??4.73 ??3.71 ??3.28 ??4.7 ??2.29 ????3.22 ???2.17 ??2.50 ???2.8
Apparent density is than (%) ??36.7 ??33.3 ??30.8 ??23.3 ??32.9 ??33.8 ????36.3 ???23.8 ??30.0 ???36.0
Bulk density is than (%) ??64.2 ??62.3 ??48.8 ??43.2 ??61.8 ??58.8 ????64.5 ???43.4 ??50.1 ???56.0
Median diameter (μ m) ??15.5 ??12.3 ??57.4 ??17.9 ??75.2 ??7.49 ????8.89 ???12.3 ??27.9 ???60.5
The ratio of the refining metallic powder in metal dust (%) 10 μ m or littler ???28 ??47 ???- ??23 ???- ??62 ????38 ???38 ????- ?????-
5 μ m or littler ???10 ??25 ???- ??7 ???- ??26 ????15 ???15 ????- ?????-
1 μ m or littler ??0.02 ??0.15 ???- ??0 ???- ??0.42 ????0 ???0 ????- ?????-
Geometric standard deviation ??2.24 ??2.07 ??2.79 ??2.57 ??2.8 ??2.19 ????2.07 ???2.79 ???2.87 ????2.9
Specific area (cm 2/g) ??1700 ??2100 ??590 ??2500 ??320 ??3700 ????3400 ???3500 ???1100 ????450
Oxygen content (%) ??0.67 ??0.78 ??0.51 ??1.08 ??1.51 ??0.18 ????0.17 ???0.17 ???0.09 ????0.12
Productive rate (%) ??86.7 ??95.1 ??45.2 ??82.3 ??36.2 ??94.5 ????90.3 ???84.1 ???44.1 ????33.2
The figure number of the powder that amplifies with Electronic Speculum ??(e) ???- ???- ???(f) ???- ???(g) ?????- ????(h) ????- ??????-

Claims (7)

1. one kind by blowing the method that a kind of cold liquid prepares metal dust to the motlten metal stream that flows down, and it is characterized in that
Cooling liquid flows to motlten metal stream downwards continuously from nozzle ring, flow around motlten metal with the bi-curved formal ring of one deck, wherein nozzle ring have hole that a motlten metal stream can pass through and
Near the constriction of this layer hyperboloid the inside, bi-curved pressure reduces by 50~750mmHg.
2. the method for claim 1 is characterized in that cooling liquid is that 1 °≤ω≤20 ° and angle of depression θ are that the direction of 5 °≤θ≤60 ° flows out with vortex angle ω.
3. by the metal dust of claim 1 or the preparation of 2 described methods, the intermediate value that it is characterized in that particle size is 50 μ m or lower, geometric standard deviation be 2.5 or lower and shape be spherical.
4. the device of preparation metal dust has one and is used for cooling liquid is blown into the nozzle ring that motlten metal flows continuously downwards, it is characterized in that:
The hole that nozzle ring has a motlten metal stream to pass through, a vortex chamber that makes cooling liquid around the hole vortex, a belt slit, cooling liquid at the vortex chamber vortex can flow to motlten metal stream from this slit after by the hole, a comb that stretches out downwards from the nozzle bottom surface of going in ring, the cooling liquid of discharging from nozzle ring can pass through this comb
The cooling liquid of discharging from narrow annular channel in comb can be centered around motlten metal stream with the bi-curved form of one deck, and like this, hyperboloid can have the pressure of 50-750mmHg to fall near the constriction in the middle of one deck is bi-curved.
5. the device of preparation metal dust as claimed in claim 4 is characterized in that comb has a vertical section through the comb axis, and its central fore-and-aft vertical plane has a chamfered portion that stretches out away from axis downwards, eliminates or prevent the collision of cold fluid and comb inwall.
6. the device of preparation metal dust as claimed in claim 5, it is characterized in that in comb, having settled a rectification body that main is arranged along the bi-curved inside of one deck that in comb, forms than lower part, wherein, the cross section of main is bigger than the constriction of hyperbolic surface layer, thereby prevents that cooling liquid from passing through comb from the turbulent flow that forms.
7. the device of preparation metal dust as claimed in claim 4, it is characterized in that the axis of the longitudinal section of comb by comb, its central fore-and-aft vertical plane has one to stretch out and be used for eliminating the chamfered portion of liquid collision and another away from axis and stretch out chamfered portion near axis downwards downwards.
CNB998014036A 1998-12-24 1999-06-23 Method of manufacturing metal powder Expired - Lifetime CN100364700C (en)

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